CN115744832A - Hydrogen peroxide purification device and purification method - Google Patents
Hydrogen peroxide purification device and purification method Download PDFInfo
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- CN115744832A CN115744832A CN202211427019.5A CN202211427019A CN115744832A CN 115744832 A CN115744832 A CN 115744832A CN 202211427019 A CN202211427019 A CN 202211427019A CN 115744832 A CN115744832 A CN 115744832A
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 404
- 238000000746 purification Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 20
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- 238000001223 reverse osmosis Methods 0.000 claims abstract description 85
- 239000011347 resin Substances 0.000 claims abstract description 36
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 32
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- 230000000149 penetrating effect Effects 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 13
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 12
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- JLLMDXDAVKMMEG-UHFFFAOYSA-N hydrogen peroxide phosphoric acid Chemical compound OO.OP(O)(O)=O JLLMDXDAVKMMEG-UHFFFAOYSA-N 0.000 claims abstract description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 66
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
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- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 6
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Abstract
A hydrogen peroxide purification device and a purification method thereof comprise a concentration device, a heat exchanger (1), a primary reverse osmosis mechanism (2), a secondary reverse osmosis mechanism (3), an ultraviolet TOC removal mechanism (4), a resin adsorption tank (5), a filter (6) and a purified hydrogen peroxide storage tank (7); concentrating industrial-grade hydrogen peroxide by a concentration device, cooling, then sending to a first-stage reverse osmosis mechanism for membrane separation, sending penetrating fluid separated from the first-stage reverse osmosis mechanism for membrane separation by a second-stage reverse osmosis mechanism, removing TOC by ultraviolet rays from the penetrating fluid separated from the second-stage reverse osmosis mechanism for digestion, then sending to a resin adsorption tank for ion exchange resin purification, discharging gas in hydrogen peroxide in the resin adsorption tank during the purification process of the ion exchange resin, adding phosphate hydrogen peroxide stabilizer into the hydrogen peroxide purified by the ion exchange resin, filtering by a filter, and then sending to a purified hydrogen peroxide storage tank for storage.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a hydrogen peroxide purification method; the invention also relates to a hydrogen peroxide purification device.
Background
The aqueous hydrogen peroxide solution is also called hydrogen peroxide, is an important raw material for producing peroxides such as peroxyacetic acid, thiourea peroxide and the like, and is also widely used in the industries such as medicine, textile printing and dyeing, papermaking bleaching and the like. The high-concentration hydrogen peroxide has strong oxidizing property and instability, is a transparent colorless liquid at normal temperature, has pungent smell, has viscosity slightly larger than water, belongs to class A fire hazard dangerous goods, and is mainly characterized by combustion supporting property, easy decomposition to generate water and oxygen.
At present, the hydrogen peroxide produced at home and abroad mostly adopts an anthraquinone method, a small amount of anthraquinone organic matters are generated in the hydrogen peroxide production process, and along with the increase of the operation time of the device, the content of the anthraquinone organic matters is also increased and is converted into the content of organic carbon which is generally below 300ppm, but along with the extension of the operation time of the device, the content of the anthraquinone organic matters can sometimes reach 400ppm or even higher.
The organic carbon in hydrogen peroxide can seriously affect the quality of products, such as: in the production process of caprolactam, if hydrogen peroxide with excessive organic carbon content is used, the organic matter can be brought into the caprolactam which is the final product, and the product purity is influenced, so that the requirement on the organic carbon content in the hydrogen peroxide in the production process of caprolactam is reduced to below 50 ppm. The electronic grade hydrogen peroxide directly affects the performance of the integrated circuit and the continuity and stability of the production thereof, and also requires higher purity.
Since the 50's of the 20 th century, many purification methods, summarized as rectification, adsorption, ion exchange, extraction, crystallization, membrane separation, and combinations thereof, have been developed in succession in order to remove impurities from hydrogen peroxide.
CN 112062096A discloses a production device and a production method of an electronic-grade hydrogen peroxide aqueous solution. The production device of the electronic-grade hydrogen peroxide water solution comprises a rectifying device, a first delivery pump, a reverse osmosis device, a second delivery pump, an ion exchange device, a third delivery pump, an ultra-pure filtering device, a fourth delivery pump and a filling device which are sequentially connected through pipelines. Rectifying industrial hydrogen peroxide, performing reverse osmosis and ion exchange, and finally filtering through an ultrafiltration membrane to obtain the electronic-grade hydrogen peroxide aqueous solution.
CN113912019A discloses a production method of an electronic-grade aqueous hydrogen peroxide solution, wherein a part of the aqueous hydrogen peroxide solution enters from the top of an evaporator, the aqueous hydrogen peroxide solution is heated by the evaporator and then enters a concentrated solution storage area of the evaporator, gas generated in the concentrated solution storage area enters a rectifying tower, the rest part of the aqueous hydrogen peroxide solution enters the rectifying tower from a second feed inlet of the rectifying tower, a part of the aqueous hydrogen peroxide solution which is concentrated and then combined by the evaporator and the rectifying tower is pumped into a heat exchanger, the aqueous hydrogen peroxide solution is cooled to normal temperature and then enters a first-grade reverse osmosis mechanism, reverse osmosis liquid obtained by reverse osmosis of the first-grade reverse osmosis mechanism enters a second-grade reverse osmosis mechanism, and reverse osmosis liquid obtained by reverse osmosis of the second-grade reverse osmosis mechanism is subjected to ion exchange by an ion exchange device to prepare the electronic-grade aqueous hydrogen peroxide solution.
The hydrogen peroxide purification method is currently applied in industry by a rectification method and a resin purification method. The rectification method is generally used for concentrating hydrogen peroxide, and because organic matters have higher boiling points, the organic matters are enriched in unvaporized liquid and are removed, so that the hydrogen peroxide is purified. However, because the gas-liquid separation is incomplete and the mist liquid is carried, volatile organic matters enter a rectification system along with hydrogen peroxide steam, the purity is generally not very high, and the production cost is high. In the hydrogen peroxide purification process, a reverse osmosis membrane separation technology is applied, so that charged ions, inorganic matters, colloidal particles and the like in the hydrogen peroxide can be effectively removed; the purification by ion exchange resin can remove not only organic carbon but also part of metal impurity ions. However, in practical application, colloidal solids are easily generated, which causes problems such as resin blockage and the like, and problems such as high treatment cost, poor separation effect, purity not meeting the requirement and the like are also caused.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a hydrogen peroxide purification device and a hydrogen peroxide purification method, which can reduce the load of resin for adsorbing organic carbon and reduce the problems of resin blockage and the like; can effectively remove charged ions, inorganic matters, colloidal particles and the like in the reverse osmosis high-salinity water, and improve the quality of the sold hydrogen peroxide.
In order to solve the above technical problems, in one aspect, the present invention provides a method for purifying hydrogen peroxide, comprising the following steps: concentrating industrial-grade hydrogen peroxide by a concentrating device, cooling, then conveying to a first-stage reverse osmosis mechanism for membrane separation, conveying a penetrating fluid separated from the first-stage reverse osmosis mechanism for membrane separation of a second-stage reverse osmosis mechanism, removing TOC (total organic carbon) from the penetrating fluid separated from the second-stage reverse osmosis mechanism by ultraviolet rays, then conveying to a resin adsorption tank for ion exchange resin purification, discharging gas in hydrogen peroxide in the process of purifying the ion exchange resin in the resin adsorption tank, adding a phosphate hydrogen peroxide stabilizer into the hydrogen peroxide purified by the ion exchange resin, filtering by a filter, and then conveying to a purified hydrogen peroxide storage tank for storage; the ultraviolet TOC removing mechanism adopts ultraviolet light with the wavelength of 185 nm; high-salt water generated by the first-stage reverse osmosis mechanism and the second-stage reverse osmosis mechanism is mixed with an oxidizing liquid of an oxidizing liquid tank and then is sent to an extraction tower, countercurrent extraction is carried out in the extraction tower by using a pure water and phosphoric acid mixed solution, raffinate enters a raffinate treatment system, extract is sent to a purification tower, countercurrent extraction is carried out in the purification tower by using heavy aromatic hydrocarbon, the heavy aromatic hydrocarbon coming out of the top of the purification tower is sent to a heavy aromatic hydrocarbon recovery system, and hydrogen peroxide coming out of the bottom of the purification tower is sent to an industrial hydrogen peroxide storage tank group for storage.
In order to solve the above technical problems, in another aspect, the present invention provides a hydrogen peroxide purification apparatus, including a concentration device for concentrating industrial-grade hydrogen peroxide, a heat exchanger for cooling the hydrogen peroxide concentrated by the concentration device, a primary reverse osmosis mechanism communicated with a hydrogen peroxide outlet of the heat exchanger, a secondary reverse osmosis mechanism having a liquid inlet communicated with a penetrating fluid outlet of the primary reverse osmosis mechanism, an ultraviolet TOC removal mechanism having a liquid inlet communicated with a penetrating fluid outlet of the secondary reverse osmosis mechanism, a resin adsorption tank having a liquid inlet communicated with a liquid outlet of the ultraviolet TOC removal mechanism, a filter having a liquid inlet communicated with a liquid outlet of the resin adsorption tank, and a hydrogen peroxide purification storage tank for storing purified hydrogen peroxide prepared by passing through the filter; the top of the resin adsorption tank is provided with an exhaust mechanism; the exhaust mechanism comprises a valve body connected with the top of the resin adsorption tank, a valve seat arranged at the lower part of the valve body, and a valve core positioned above the valve seat; still include the oxidation cistern, the extraction tower, the purifying column, the high salt water export of one-level reverse osmosis mechanism, the high salt water export of second grade reverse osmosis mechanism and the oxidation liquid export of oxidation cistern all through the pipeline with the bottom inlet of extraction tower is connected, the top inlet and the pure water feeding mechanism of extraction tower are connected, the bottom liquid outlet of extraction tower pass through the pipeline with the top inlet of purifying column is connected, the top raffinate export of extraction tower passes through the pipeline and is connected with raffinate processing system, the bottom inlet and the heavy aromatics of purifying column come the charging tube and are connected, the top liquid outlet of purifying column passes through the pipeline and is connected with heavy aromatics recovery system, the bottom liquid outlet of purifying column passes through pipeline and industrial grade hydrogen peroxide solution basin group link.
As a further improved technical scheme, the ultraviolet TOC removing mechanism of the hydrogen peroxide purifying device provided by the invention adopts ultraviolet light with the wavelength of 185 nm.
As a further improved technical scheme, the hydrogen peroxide purification device provided by the invention comprises a rectifying tower, a condenser connected with a steam outlet of the rectifying tower through a pipeline, a cyclone separator connected with a non-condensable gas outlet of the condenser through a pipeline, a jet vacuum pump connected with a gas outlet of the cyclone separator through a pipeline, a gas-liquid separator connected with the jet vacuum pump through a pipeline, a roots vacuum pump connected with a gas outlet of the gas-liquid separator through a pipeline, a water ring vacuum pump connected with the roots vacuum pump in series, a circulating water tank connected with a liquid outlet of the gas-liquid separator through a pipeline, and a circulating pump connected with the circulating water tank through a pipeline and used for conveying circulating water to the jet vacuum pump.
As a further improved technical scheme, the hydrogen peroxide purification device provided by the invention comprises a purified hydrogen peroxide storage tank, a liquid inlet connected with the upper part or the top of the purified hydrogen peroxide storage tank, a liquid outlet connected with the lower part or the bottom of the purified hydrogen peroxide storage tank, a collecting tank surrounding the upper part of the inner wall of the purified hydrogen peroxide storage tank and connected with the purified hydrogen peroxide storage tank, a liquid discharge pipe with a first end communicated with the collecting tank, a hydrogen peroxide condensate collecting storage tank connected with the other end of the liquid discharge pipe, and at least one breathing pipe connected with the purified hydrogen peroxide storage tank, the hydrogen peroxide condensate collecting storage tank or the liquid discharge pipe; the inner wall of the top of the purified hydrogen peroxide storage tank is conical or hemispherical; the cross section of the collecting tank is semicircular or arc-shaped, and the lowest part of the outer bottom surface of the collecting tank is positioned on the inner side of the polytetrafluoroethylene layer; a second polytetrafluoroethylene layer is lined on the outer bottom surface of the collecting tank, the top end of the polytetrafluoroethylene layer is inserted into a connecting gap between the collecting tank and the purified hydrogen peroxide storage tank, one end of the second polytetrafluoroethylene layer wraps the tank edge of the collecting tank, and the other end of the second polytetrafluoroethylene layer is inserted into the polytetrafluoroethylene layer at the connecting position of the polytetrafluoroethylene layer and the collecting tank; the top of the second polytetrafluoroethylene layer has a slope that slopes into the collection trough.
As a further improved technical scheme, the hydrogen peroxide purification device provided by the invention is characterized in that the industrial-grade hydrogen peroxide storage tank set comprises a first hydrogen peroxide storage tank, an adjusting valve with an outlet end communicated with the first hydrogen peroxide storage tank, a gas filter with an outlet end communicated with an inlet end of the adjusting valve, a pressure reducing valve with an outlet end communicated with an inlet end of the gas filter, a nitrogen gas supply pipe communicated with an inlet end of the pressure reducing valve, at least one hydrogen peroxide storage tank connected with the first hydrogen peroxide storage tank in series through a nitrogen gas pipeline, a nitrogen gas discharge pipe communicated with the hydrogen peroxide storage tank connected with the tail of the series, and a water seal tank; the nitrogen gas discharge pipe is inserted into the water seal tank.
As a further improved technical scheme, the hydrogen peroxide purification device provided by the invention further comprises a first control valve connected with a concentrated solution outlet pipeline of the primary reverse osmosis mechanism and a second control valve connected with a concentrated solution outlet pipeline of the secondary reverse osmosis mechanism.
The aforementioned improvements can be implemented individually or in combination without conflict.
According to the technical scheme provided by the invention, industrial-grade hydrogen peroxide passes through a primary reverse osmosis mechanism 2 and a secondary reverse osmosis mechanism 3, water and the hydrogen peroxide pass through a reverse osmosis membrane of the secondary reverse osmosis mechanism 3 and then enter an ultraviolet TOC removing mechanism 4, are irradiated by ultraviolet light with the wavelength of 185nm, are digested to remove partial TOC (total organic carbon) and then enter a resin adsorption tank 5 to further remove organic carbon and partial metal ion impurities, and the resin adsorption tank 5 timely oxidizes CO generated by organic matters 2 And the gas decomposed by hydrogen peroxide is discharged, so that the normal production of the resin adsorption tank is maintained, and the purified hydrogen peroxide which can be stably stored is obtained after the stabilizer is added and filtered by the filter 6.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a schematic view of the hydrogen peroxide purification apparatus according to the embodiment;
FIG. 2 is a schematic view of the structure of a storage tank for purified hydrogen peroxide in the example;
FIG. 3 isbase:Sub>A schematic view of the structure in the direction A-A in FIG. 2;
FIG. 4 is an enlarged view of portion B of FIG. 2;
FIG. 5 is a schematic view of the structure of a resin adsorption tank in the example;
FIG. 6 is an enlarged view of section C of FIG. 5;
fig. 7 is a schematic structural diagram of an industrial-grade hydrogen peroxide storage tank set in the embodiment.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
The hydrogen peroxide purification device shown in fig. 1 comprises a concentration device for concentrating industrial-grade hydrogen peroxide, a heat exchanger 1 for cooling the hydrogen peroxide concentrated by the concentration device, a primary reverse osmosis mechanism 2 communicated with a hydrogen peroxide outlet of the heat exchanger 1, a secondary reverse osmosis mechanism 3 with a liquid inlet communicated with a penetrating fluid outlet of the primary reverse osmosis mechanism 2, an ultraviolet TOC removal mechanism 4 with a liquid inlet communicated with a penetrating fluid outlet of the secondary reverse osmosis mechanism 3, a resin adsorption tank 5 with a liquid inlet communicated with a liquid outlet of the ultraviolet TOC removal mechanism 4, a filter 6 with a liquid inlet communicated with a liquid outlet of the resin adsorption tank 5, and a purified hydrogen peroxide storage tank 7 for storing purified hydrogen peroxide prepared after passing through the filter 6; as shown in fig. 5 and 6, the top of the resin adsorption tank 5 is provided with a gas exhaust mechanism; the exhaust mechanism comprises a valve body 39 connected with the top of the resin adsorption tank 5, a valve seat 40 arranged at the lower part of the valve body 39, and a valve core 41 positioned above the valve seat; as shown in fig. 1, the hydrogen peroxide solution purification apparatus further includes an oxidation liquid tank 8, an extraction tower 9 and a purification tower 10, wherein a high-salt water outlet of the first-level reverse osmosis mechanism 2, a high-salt water outlet of the second-level reverse osmosis mechanism 3 and an oxidation liquid outlet of the oxidation liquid tank 8 are connected to a bottom liquid inlet of the extraction tower 9 through pipelines, a top liquid inlet of the extraction tower 9 is connected to a pure water supply device, a bottom liquid outlet of the extraction tower 9 is connected to a top liquid inlet of the purification tower 10 through a pipeline, a top raffinate outlet of the extraction tower 9 is connected to a raffinate treatment system through a pipeline, a bottom liquid inlet of the purification tower 10 is connected to a heavy aromatic hydrocarbon supply pipe, a top liquid outlet of the purification tower 10 is connected to a heavy aromatic hydrocarbon recovery system through a pipeline, and a bottom liquid outlet of the purification tower 10 is connected to an industrial hydrogen peroxide solution storage tank through a pipeline. The extraction tower 9 is a sieve plate tower, the purification tower 10 is a packed tower, and the heavy aromatic hydrocarbon is C9 and C10 aromatic hydrocarbon.
The industrial-grade hydrogen peroxide with the concentration of 27.5wt% -33 wt% in the industrial-grade hydrogen peroxide storage tank set is concentrated by a concentration device until the concentration of the aqueous solution of the hydrogen peroxide is not lower than 50wt%, the aqueous solution is cooled to normal temperature by a heat exchanger 1 and then enters a first-grade reverse osmosis mechanism 2 for membrane separation, reverse osmosis liquid obtained after the membrane separation of the first-grade reverse osmosis mechanism 2 enters a second-grade reverse osmosis mechanism 3, the reverse osmosis liquid obtained after the membrane separation of the second-grade reverse osmosis mechanism 3 is sent to an ultraviolet TOC removal mechanism 4, and organic matters in the hydrogen peroxide are oxidized into CO by ultraviolet rays 2 And H 2 Removing TOC by ultraviolet ray, removing by a TOC mechanism 4, purifying by ion exchange resin in a resin adsorption tank 5, adding phosphate peroxide into the hydrogen peroxide purified by the ion exchange resinThe hydrogen stabilizer is filtered by a filter 6 and then sent to a purified hydrogen peroxide storage tank 7 for storage. The ultraviolet light TOC removal mechanism 4 employs ultraviolet light having a wavelength of 185 nm. After the gas in the resin adsorption tank 5 is gathered to generate pressure, the valve core 41 overcomes the action of gravity after being subjected to the pressure action of the gas, the valve core 41 is lifted, a gap is generated between the valve seat 40 and the valve core 41, the gas in the resin adsorption tank 5 is discharged, and after the gas is discharged and reduced in pressure, the valve core 41 descends and resets under the action of gravity. CO generated by oxidizing organic matters in hydrogen peroxide 2 And gas generated by hydrogen peroxide decomposition is discharged in time, so that the normal production of the resin adsorption tank is maintained. The high-salt water generated by the first-stage reverse osmosis mechanism 2 and the second-stage reverse osmosis mechanism 3 is mixed with the oxidation liquid of an oxidation liquid tank 8 of an anthraquinone process hydrogen peroxide production line and then is sent into an extraction tower 9, the extraction tower 9 is subjected to countercurrent extraction by using a mixed solution of pure water and phosphoric acid, raffinate enters a raffinate treatment system, extract is sent into a purification tower 10, C9 and C10 heavy aromatics are subjected to countercurrent extraction in the purification tower 10, the heavy aromatics coming out of the top of the purification tower are sent to a heavy aromatics recovery system, and hydrogen peroxide coming out of the bottom of the purification tower 10 is sent to an industrial hydrogen peroxide storage tank set for storage.
And the oxidation liquid in the oxidation liquid tank 8 of the anthraquinone method hydrogen peroxide production line, the high-salt water of the first-stage reverse osmosis mechanism 2 and the high-salt water of the second-stage reverse osmosis mechanism 3 are sent to the extraction tower 9 through oxidation liquid pumps. The oxidizing liquid containing hydrogen peroxide and the high-salt water are dispersed into innumerable small oil droplets and float to the top of the extraction tower after entering from the bottom of the extraction tower 9, and at the same time, the pure water supply means mixes the pure water with the phosphoric acid solution and sends the extraction water to the top of the extraction tower 9, and the extraction water continuously flows downward and is subjected to counter-current extraction with the oxidizing liquid and the high-salt water floating upward. In the extraction process, water is used as a continuous phase, and the oxidizing solution and the high-salt water are used as dispersed phases. During the process of the extraction water flowing from the top to the bottom of the tower, the hydrogen peroxide content gradually increases, and finally the extraction water flows out from the bottom of the tower, which is called extraction liquid (crude hydrogen peroxide), and enters the top of the purification tower 10 through a potential difference. The oxidation liquid and the high salt water entering from the bottom of the extraction tower 9 are dispersed and float upwards, the hydrogen peroxide content is gradually reduced, and finally the oxidation liquid and the high salt water flow out from the top of the tower, and the oxidation liquid and the high salt water are called raffinate, and the raffinate enters a raffinate treatment system after being separated. Charged ions, inorganic matters, colloidal particles and the like in the reverse osmosis high-salinity water enter the raffinate and are removed.
The extract liquid contains a small amount of working fluid and organic substances, and a purification treatment is required to remove these impurities. The purifying tower 10 is filled with C9 and C10 heavy aromatics, the extract liquid entering from the top of the tower flows downwards in the tower, the C9 and C10 heavy aromatics are pumped into the bottom of the purifying tower 10 by an aromatic hydrocarbon pump to form countercurrent extraction with the extract liquid so as to remove organic impurities in the hydrogen peroxide, and in the process, the heavy aromatics are a continuous phase and the extract liquid is a disperse phase. Organic matters in the hydrogen peroxide are removed. The purified hydrogen peroxide flows out from the bottom of the purification tower 10 and enters an industrial-grade hydrogen peroxide storage tank set.
The reverse osmosis membranes of the first-stage reverse osmosis mechanism 2 and the second-stage reverse osmosis mechanism 3 can adopt aromatic polyamide membranes, polyamide piperazine membranes, polysulfone membranes, polyvinyl chloride membranes and the like, under the action of pressure, water and small molecular substances of hydrogen peroxide can pass through the reverse osmosis membranes, and charged ions, inorganic substances with larger molecular weight and colloidal particles cannot pass through the reverse osmosis membranes, so that the hydrogen peroxide solution at the penetrating fluid outlet of the reverse osmosis mechanism can effectively remove the charged ions, the inorganic substances with larger molecular weight and the colloidal particles, thereby improving the purity of the hydrogen peroxide solution. The ultraviolet TOC removal means 4 uses ultraviolet light having a wavelength of 185nm, the energy of which promotes the formation of radicals and the oxidation of organic substances to CO 2 And H 2 And O. TOC (Total organic carbon) is eliminated. The hydrogen peroxide is purified by ion exchange resin in the resin adsorption tank 5, and not only organic carbon but also a part of metal ion impurities can be removed. After the hydrogen peroxide passes through the resin adsorption tank 5, the stabilizing agent is added, and then the hydrogen peroxide is filtered by the filter 6, so that solid matters in the stabilizing agent can be filtered.
According to the technical scheme provided by the invention, industrial-grade hydrogen peroxide passes through a primary reverse osmosis mechanism 2 and a secondary reverse osmosis mechanism 3, water and the hydrogen peroxide pass through a reverse osmosis membrane of the secondary reverse osmosis mechanism 3 and then enter an ultraviolet TOC removing mechanism 4, and are irradiated by ultraviolet light with the wavelength of 185nm to clear up and remove partial TOC (total organic carbon) and then enter resin for absorptionThe attached tank 5 further removes organic carbon and partial metal ion impurities, and the resin adsorption tank 5 timely oxidizes the organic matters to generate CO 2 And the gas decomposed by hydrogen peroxide is discharged, so that the normal production of the resin adsorption tank is maintained, and the purified hydrogen peroxide which can be stably stored is obtained after the stabilizer is added and filtered by the filter 6.
As an embodiment thereof, the hydrogen peroxide purification apparatus provided by the present invention, as shown in fig. 1, includes a rectifying tower 11, a condenser 12 connected to a steam outlet of the rectifying tower 11 through a pipeline, a cyclone 13 connected to a non-condensable gas outlet of the condenser 12 through a pipeline, a jet vacuum pump 14 connected to a gas outlet of the cyclone 13 through a pipeline, a gas-liquid separator 15 connected to the jet vacuum pump 14 through a pipeline, a roots vacuum pump 16 connected to an air outlet of the gas-liquid separator 15 through a pipeline, a water ring vacuum pump 17 connected in series with the roots vacuum pump 16, a circulating water tank 18 connected to a liquid outlet of the gas-liquid separator 15 through a pipeline, and a circulating pump 19 connected to the circulating water tank 18 through a pipeline and supplying circulating water to the jet vacuum pump 14.
After steam generated by the rectifying tower 11 passes through the condenser 12, water and hydrogen peroxide are discharged from a condensate discharge pipe of the condenser 12, non-condensable gas and a small amount of entrained liquid enter the cyclone separator 13, the non-condensable gas separated by the cyclone separator 13 enters the jet vacuum pump 14, and then the non-condensable gas is discharged through the roots vacuum pump 16 or the water ring vacuum pump 17. The injection liquid of the injection vacuum pump 14 can absorb the uncondensed hydrogen peroxide, and the hydrogen peroxide absorbed in the injection liquid can be recycled. The roots vacuum pump 16 can discharge a large amount of non-condensable gas out of the system, while the water ring vacuum pump 17 can significantly increase the degree of vacuum of the system although the amount of gas discharged is not large. The combination of the jet vacuum pump 14, the Roots vacuum pump 16 and the water-ring vacuum pump 17 is beneficial to improving the vacuum degree of the system, reducing the energy consumption and recycling the hydrogen peroxide carried in the non-condensable gas.
As an embodiment of the hydrogen peroxide purification apparatus, the purified hydrogen peroxide storage tank shown in fig. 2 to 4 includes a purified hydrogen peroxide storage tank 20, a liquid inlet 21 connected to an upper portion or a top portion of the purified hydrogen peroxide storage tank 20, a liquid outlet 22 connected to a lower portion or a bottom portion of the purified hydrogen peroxide storage tank 20, a collecting tank 23 surrounding an upper portion of an inner wall of the purified hydrogen peroxide storage tank 20 and connected to the purified hydrogen peroxide storage tank 20, a liquid discharge pipe 24 having a first end connected to the collecting tank 23, a hydrogen peroxide condensate collecting storage tank 25 connected to another end of the liquid discharge pipe 24, and at least one breathing pipe 26 connected to the purified hydrogen peroxide storage tank 20, the hydrogen peroxide condensate collecting storage tank 25, or the liquid discharge pipe 24; a polytetrafluoroethylene layer 27 is lined below the collecting tank 23 of the purified hydrogen peroxide storage tank 20, and the inner wall of the top of the purified hydrogen peroxide storage tank 20 is conical or hemispherical; the section of the collecting tank 23 is semicircular or arc-shaped, and the lowest position of the outer bottom surface of the collecting tank 23 is positioned on the inner side of the polytetrafluoroethylene layer 27; a second polytetrafluoroethylene layer 28 is lined on the outer bottom surface of the collecting tank 23, the top end of the polytetrafluoroethylene layer 27 is inserted into a connecting gap between the collecting tank 23 and the purified hydrogen peroxide storage tank 20, one end of the second polytetrafluoroethylene layer 28 wraps the tank edge of the collecting tank 23, and the other end of the second polytetrafluoroethylene layer 28 is inserted into the polytetrafluoroethylene layer 27 at the connecting position of the polytetrafluoroethylene layer 27 and the collecting tank 23; the top of the second ptfe layer 28 has a sloping surface 29 sloping into the collection trough 23.
The main structure of the hydrogen peroxide storage tank is a stainless steel storage tank and lined with polytetrafluoroethylene, if the construction difficulty of lining the polytetrafluoroethylene at the top of the purified hydrogen peroxide storage tank 20 is very high, the structure is unstable, the polytetrafluoroethylene layer 27 lined below the collecting tank 23 of the purified hydrogen peroxide storage tank 20 can be selected to avoid direct contact of hydrogen peroxide and hydrogen peroxide, and the construction has feasibility. The hydrogen peroxide can produce hydrogen peroxide steam and vapor in the storage process, the steam rises to the top of the purified hydrogen peroxide storage tank 20 and condenses, the condensed liquid drops are attached to the inner wall of the top of the purified hydrogen peroxide storage tank 20, and the condensed water at the top contacts the wall of the metal tank, so that metal impurities are contained in the condensed water, and if the condensed water is mixed into the purified hydrogen peroxide, the product is unqualified. According to the technical scheme provided by the invention, the condensed water on the top part flows into the collecting tank 23 along the inner wall of the top part after being collected, and then flows into the hydrogen peroxide condensate collecting storage tank 25 from the collecting tank 23 through the liquid discharge pipe 24, so that the pollution of the purified hydrogen peroxide caused by the condensed water dropping on the top of the tank is avoided, and the risk of impurities mixed in the purified hydrogen peroxide in the storage process is reduced. The lowest position of the outer bottom surface of the collecting tank 23 is located on the inner side of the polytetrafluoroethylene layer 27, so that liquid drops can be prevented from entering between the main body layer of the purified hydrogen peroxide storage tank 20 and the polytetrafluoroethylene layer 27, and the hydrogen peroxide is prevented from corroding the main body layer of the purified hydrogen peroxide. A second polytetrafluoroethylene layer 28 is lined on the outer bottom surface of the collecting tank 23, the top end of the polytetrafluoroethylene layer 27 is inserted into a connecting gap between the collecting tank 23 and the purified hydrogen peroxide storage tank 20, one end of the second polytetrafluoroethylene layer 28 wraps the tank edge of the collecting tank 23, and the other end of the second polytetrafluoroethylene layer is inserted into the polytetrafluoroethylene layer 27 at the connecting part of the polytetrafluoroethylene layer 27 and the collecting tank 23; the design scheme that the inclined plane 29 inclining towards the inside of the collecting groove 23 is arranged at the top of the second polytetrafluoroethylene layer 28 can prevent condensed liquid drops from entering between the main body layer of the purified hydrogen peroxide storage tank 20 and the polytetrafluoroethylene layer 27 and entering between the collecting groove 23 and the second polytetrafluoroethylene layer 28, and can also prevent the condensed water drops on the bottom surface of the collecting groove 23 from polluting the purified hydrogen peroxide.
As an embodiment of the hydrogen peroxide purification apparatus provided by the present invention, as shown in fig. 7, an industrial-grade hydrogen peroxide storage tank set includes a first hydrogen peroxide storage tank 30, an adjusting valve 31 having an outlet end communicated with the first hydrogen peroxide storage tank 30, a gas filter 32 having an outlet end communicated with an inlet end of the adjusting valve 31, a pressure reducing valve 33 having an outlet end communicated with an inlet end of the gas filter 32, a nitrogen gas supply pipe communicated with an inlet end of the pressure reducing valve 33, at least one hydrogen peroxide storage tank 34 connected in series with the first hydrogen peroxide storage tank 30 through a nitrogen gas pipeline, a nitrogen gas discharge pipe 35 connected with the hydrogen peroxide storage tank 34 connected in series with the tail end of the first hydrogen peroxide storage tank, and a water seal tank 36; the nitrogen gas discharge pipe 35 is inserted into the water seal tank 36.
The compressed nitrogen is decompressed by a decompression valve 33, enters the top of the first hydrogen peroxide storage tank 30 after passing through a gas filter 32, sequentially enters the hydrogen peroxide storage tanks 34 which are connected in series from the top of the first hydrogen peroxide storage tank 30, enters the water seal tank 36 from a nitrogen discharge pipe 35 of the hydrogen peroxide storage tank 34 which is connected in series and arranged at the tail, and finally overflows from the water seal tank 36. The nitrogen enters the hydrogen peroxide storage tanks connected in series in sequence and is sealed by the water seal tanks, so that the nitrogen seal effect of the hydrogen peroxide storage tank can be improved, and the consumption of the nitrogen is reduced.
As an embodiment, as shown in fig. 1, the hydrogen peroxide purification apparatus provided by the present invention further includes a first control valve 37 connected to the concentrated solution outlet pipeline of the primary reverse osmosis mechanism 2, and a second control valve 38 connected to the concentrated solution outlet pipeline of the secondary reverse osmosis mechanism 3.
The concentrated solution outlet pipelines of the first-stage reverse osmosis mechanism 2 and the second-stage reverse osmosis mechanism 3 are provided with control valves, so that the production can be conveniently and flexibly adjusted, the reverse osmosis pressure of the reverse osmosis mechanism is guaranteed through pressure control, the production is carried out under stable reverse osmosis pressure, the production efficiency can be improved, and the reverse osmosis mechanism is prevented from operating at overpressure.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention in any way, and various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A hydrogen peroxide purification method is characterized by comprising the following steps: concentrating industrial-grade hydrogen peroxide by a concentration device, cooling, then conveying to a first-stage reverse osmosis mechanism for membrane separation, conveying penetrating fluid separated from the first-stage reverse osmosis mechanism for membrane separation by a second-stage reverse osmosis mechanism, digesting penetrating fluid separated from the second-stage reverse osmosis mechanism by an ultraviolet TOC removal mechanism, then conveying the penetrating fluid to a resin adsorption tank for ion exchange resin purification, discharging gas in hydrogen peroxide in the resin adsorption tank during the purification process of the ion exchange resin, adding a phosphate hydrogen peroxide stabilizer into the hydrogen peroxide purified by the ion exchange resin, filtering by a filter, and then conveying to a purified hydrogen peroxide storage tank for storage; the ultraviolet TOC removing mechanism adopts ultraviolet light with the wavelength of 185 nm; high-salt water generated by the first-stage reverse osmosis mechanism and the second-stage reverse osmosis mechanism is mixed with an oxidizing liquid in an oxidizing liquid tank and then is sent to an extraction tower, mixed liquid of pure water and phosphoric acid is used for countercurrent extraction in the extraction tower, raffinate enters a raffinate treatment system, extract is sent to a purification tower, heavy aromatic hydrocarbon is used for countercurrent extraction in the purification tower, the heavy aromatic hydrocarbon coming out of the top of the purification tower is sent to a heavy aromatic hydrocarbon recovery system, and hydrogen peroxide coming out of the bottom of the purification tower is sent to an industrial-grade hydrogen peroxide storage tank group for storage.
2. A hydrogen peroxide purification device is characterized by comprising a concentration device for concentrating industrial hydrogen peroxide, a heat exchanger (1) for cooling the concentrated hydrogen peroxide of the concentration device, a primary reverse osmosis mechanism (2) communicated with a hydrogen peroxide outlet of the heat exchanger (1), a secondary reverse osmosis mechanism (3) with a liquid inlet communicated with a penetrating fluid outlet of the primary reverse osmosis mechanism (2), an ultraviolet TOC removal mechanism (4) with a liquid inlet communicated with a penetrating fluid outlet of the secondary reverse osmosis mechanism (3), a resin adsorption tank (5) with a liquid inlet communicated with a liquid outlet of the ultraviolet TOC removal mechanism (4), a filter (6) with a liquid inlet communicated with a liquid outlet of the resin adsorption tank (5), and a purified hydrogen peroxide storage tank (7) for storing purified hydrogen peroxide prepared after passing through the filter (6); the top of the resin adsorption tank (5) is provided with an exhaust mechanism; the exhaust mechanism comprises a valve body (39) connected with the top of the resin adsorption tank (5), a valve seat (40) arranged at the lower part of the valve body (39), and a valve core (41) positioned above the valve seat; still include oxidation cistern (8), extraction tower (9), purifying column (10), the high salt water export of one-level reverse osmosis mechanism (2), second grade reverse osmosis mechanism (3) and the oxidation liquid export of oxidation cistern (8) all through the pipeline with the bottom inlet of extraction tower (9) is connected, the top inlet and the pure water feeding mechanism of extraction tower (9) are connected, the bottom liquid outlet of extraction tower (9) pass through the pipeline with the top inlet of purifying column (10) is connected, the top raffinate export of extraction tower (9) passes through pipeline and raffinate processing system connection, the bottom inlet and the heavy aromatics incoming material union coupling of purifying column (10), the top liquid outlet of purifying column (10) passes through the pipeline and is connected with heavy aromatics recovery system, the bottom of purifying column (10) passes through the liquid outlet and is connected with industrial-grade hydrogen peroxide solution storage tank group.
3. The hydrogen peroxide purification apparatus according to claim 2, wherein the ultraviolet TOC removal mechanism (4) employs ultraviolet light having a wavelength of 185 nm.
4. The hydrogen peroxide purification device according to claim 2, wherein the concentration device comprises a rectification column (11), a condenser (12) connected with a steam outlet of the rectification column (11) through a pipeline, a cyclone separator (13) connected with a non-condensable gas outlet of the condenser (12) through a pipeline, an ejector vacuum pump (14) connected with a gas outlet of the cyclone separator (13) through a pipeline, a gas-liquid separator (15) connected with the ejector vacuum pump (14) through a pipeline, a roots vacuum pump (16) connected with a gas outlet of the gas-liquid separator (15) through a pipeline, a water ring vacuum pump (17) connected with the roots vacuum pump (16) in series, a circulating water pool (18) connected with a liquid outlet of the gas-liquid separator (15) through a pipeline, and a circulating pump (19) connected with the circulating water pool (18) through a pipeline and sending circulating water to the ejector vacuum pump (14).
5. The hydrogen peroxide purification device according to claim 2, wherein the purified hydrogen peroxide storage tank comprises a purified hydrogen peroxide storage tank (20), a liquid inlet (21) connected with the upper part or the top of the purified hydrogen peroxide storage tank (20), a liquid outlet (22) connected with the lower part or the bottom of the purified hydrogen peroxide storage tank (20), a collecting tank (23) surrounding the upper part of the inner wall of the purified hydrogen peroxide storage tank (20) and connected with the purified hydrogen peroxide storage tank (20), a liquid discharge pipe (24) with a first end communicated with the collecting tank (23), a hydrogen peroxide condensate collecting storage tank (25) connected with the other end of the liquid discharge pipe (24), and at least one breathing pipe (26) connected with the purified hydrogen peroxide storage tank (20), the hydrogen peroxide condensate collecting storage tank (25) or the liquid discharge pipe (24); a polytetrafluoroethylene layer (27) is lined below the collecting tank (23) of the purified hydrogen peroxide storage tank (20), and the inner wall of the top of the purified hydrogen peroxide storage tank (20) is conical or hemispherical; the section of the collecting groove (23) is semicircular or arc-shaped, and the lowest position of the outer bottom surface of the collecting groove (23) is positioned on the inner side of the polytetrafluoroethylene layer (27); a second polytetrafluoroethylene layer (28) is lined on the outer bottom surface of the collecting tank (23), the top end of the polytetrafluoroethylene layer (27) is inserted into a connecting gap between the collecting tank (23) and the purified hydrogen peroxide storage tank (20), one end of the second polytetrafluoroethylene layer (28) wraps the tank edge of the collecting tank (23), and the other end of the second polytetrafluoroethylene layer is inserted into the polytetrafluoroethylene layer (27) at the connecting position of the polytetrafluoroethylene layer (27) and the collecting tank (23); the second polytetrafluoroethylene layer (28) has on its top a bevel (29) sloping into the collection trough (23).
6. The hydrogen peroxide purification device according to claim 2, wherein the industrial-grade hydrogen peroxide storage tank set comprises a first hydrogen peroxide storage tank (30), an adjusting valve (31) with an outlet end communicated with the first hydrogen peroxide storage tank (30), a gas filter (32) with an outlet end communicated with an inlet end of the adjusting valve (31), a pressure reducing valve (33) with an outlet end communicated with an inlet end of the gas filter (32), a nitrogen supply pipe communicated with an inlet end of the pressure reducing valve (33), at least one hydrogen peroxide storage tank (34) connected with the first hydrogen peroxide storage tank (30) in series through a nitrogen pipeline, a nitrogen discharge pipe (35) communicated with the hydrogen peroxide storage tank (34) connected with the tail of the series, and a water seal tank (36); the nitrogen gas discharge pipe (35) is inserted into the water seal tank (36).
7. The hydrogen peroxide purification device according to claim 2, further comprising a first control valve (37) connected to the concentrated liquid outlet pipeline of the primary reverse osmosis mechanism (2), and a second control valve (38) connected to the concentrated liquid outlet pipeline of the secondary reverse osmosis mechanism (3).
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